Water → Ethyl 6-[4-(7-methoxy-2-oxo-1,2,4,5-tetrahydro-1,3-benzodiazepin-3-yl)-piperidin-1-yl]-pyrimidine-4-carboxylate

HRID 74504Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 74504
[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]2[NH:12][C:11](=[O:13])[N:10]([CH:14]3[CH2:19][CH2:18][NH:17][CH2:16][CH2:15]3)[CH2:9][CH2:8][C:7]=2[CH:20]=1.CCN(C(C)C)C(C)C.Cl[C:31]1[N:36]=[CH:35][N:34]=[C:33]([C:37]([O:39][CH2:40][CH3:41])=[O:38])[CH:32]=1.O>CN(C=O)C.C(OCC)(=O)C>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]2[NH:12][C:11](=[O:13])[N:10]([CH:14]3[CH2:19][CH2:18][N:17]([C:31]4[N:36]=[CH:35][N:34]=[C:33]([C:37]([O:39][CH2:40][CH3:41])=[O:38])[CH:32]=4)[CH2:16][CH2:15]3)[CH2:9][CH2:8][C:7]=2[CH:20]=1

Komponenten

7

Edukt 4

HCID 962WaterHCID 81531DiisopropylethylamineHCID 183568527-methoxy-3-(piperidin-4-yl)-4,5-dihydro-1H-benzo[d][1,3]diazepin-2(3H)-oneHCID 22756838Ethyl 6-chloropyrimidine-4-carboxylate

Produkt 1

HCID 58386752Ethyl 6-[4-(7-methoxy-2-oxo-1,2,4,5-tetrahydro-1,3-benzodiazepin-3-yl)-piperidin-1-yl]-pyrimidine-4-carboxylate

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6228DimethylformamideLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

2.80 g (10.2 mmol) 7-methoxy-3-piperidin-4-yl-1,3,4,5-tetrahydro-1,3-benzodiazepin-2-one and 6.00 mL (34.9 mmol) DIPEA were added to 1.90 g (10.2 mmol) ethyl 6-chloropyrimidine-4-carboxylate in 60 mL DMF and the reaction mixture was stirred for 3 h at RT. After elimination of the solvent i. vac. the residue was combined with 70 mL water and stirred for 10 min. 5 mL ethyl acetate were added. After vigorous stirring the solid was suction filtered and dried in the CAD.

Aufarbeitung

  1. stirringstirred for 10 min
  2. stirringAfter vigorous stirring the solid
  3. filtrationfiltered
  4. customdried in the CAD

Quellen und Nachweise

ORD-Eintrag
ord-9cfe5f1b925142c4b3372c5a4f8eccb9
Quelldatensatz
uspto-grants-2014_09
Patentnummer
US08829006B2

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